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By J. E. Pahlman

Spontaneous oxidation and combustion of sulfides and resultant fires are serious problems in underground mines. The Bureau of Mines has con-ducted fundamental thermal gravimetric analysis (TGA) research to deter-mine the mechanisms and factors governing the rate of low-temperature pyrite oxidation, and to identify possible inhibitors to spontaneous oxidation and combustion. The mechanism of low-temperature pyrite oxidation was found to be topochemical, meaning that the oxidation process is controlled by the chemical reaction at the interface between pyrite (FeS2) and iron sulfate (FeS04)' An activation energy of 8.9 kcal/mol FeS2 was obtained for oxidation of minus 500-mesh pyrite in an atmosphere of 60 vol pct water vapor and 40 vol pct . Water-vapor content of the atmosphere was found to be the critical factor in the rate of spontaneous oxidation of pyrite, with a water-vapor content greater than 20 vol pct needed for accelerated oxidation. An atmosphere of pure oxygen resulted in negligible oxidation. The rate of pyrite oxidation is also greatly affected by the particle size of pyrite. Pyrite-oxidation rate increased drastically for particles less than 40 ~m. Room-temperature pyrophoric behavior was observed for freshly ground unoxidized pyrite (55 pct minus 5 ~m) upon exposure to air. Addition of water-adsorbing materials such as activated alumina (Alz03) decreased the rate of pyrite oxidation.

Jan 1, 1986

By Wilbur I. Duvall

The borehole deformation gage and overcoring techniques developed by the Bureau of Mines form one of the primary methods of determining in situ rock stress. This report describes a least squares method of calculating the average rock stress components in the horizontal plane from more than three diametral deformation measurements in a vertical borehole. This least squares analysis provides a means of determining the multiple correlation coefficient, the variance, and the scatter for a set of deformation measurements. From this information, confidence limits can be calculated for the secondary horizontal principal stresses and their directions. The material presented in this report can be used as a guide to the development of least squares solutions for stress measurement techniques other than the borehole deformation method. Since the statistical information that results from the least squares method is extremely useful in the interpretation of results, it is recommended that a least squares analysis be used on stress measurement data whenever possible.

Jan 1, 1979

The STATE MINERAL SUMMARIES publication provides estimated data and summaries of mineral activities at the State level for 1990. Most of the estimates are based on nine months data. These summaries have been prepared in cooperation with State geological surveys or related agencies. Individual State summaries are published separately as State Mineral Industry Surveys and copies can be obtained from the appropriate State Activities field office.

Jan 1, 1991

By E. R. Cole

This Bureau of Mines investigation was prompted by the need forr a stable anode for electrowinning metals, particularly zinc and copper, from acid solutions. The polarization behavior of Pb-Ag (1 pct Ag) anodes in H2SO4 and fluoride solutions was determined as the first step in the development of such an anode. A Luggin capillary, dc power supply, high-impedance voltmeter, and other equipment standard to an electrochemical laboratory were used in this study. It was determined that during polarization, a relatively hard, stable coating of Pb02 was formed on the surface of the lead-silver anode and the rate of formation of this coating was considerably enhanced by the presence of fluoride ions in solution. Subsequent investigations at the Bureau of Mines Rolla Research Center resulted in the development of a Pb02-coated titanium (Pb02-Ti) anode. Results of this effort were presented in Bureau of Mines Report of Investigations 8111. Additional data resulting from extensive testing of the Pb02-Ti anodes, as well as process improvements and innovations, are included in this report. The anodes were considered generally unsatisfactory for zinc electrowinning because of lower conductivity, higher oxygen overvoltages, and shorter in-cell life as compared with the Pb-Ag anodes now being used in industry. However, the PbO2-Ti anodes were used successfully to oxidize waste chromium solutions and to electrowin copper.

Jan 1, 1981

By D. E. Wolfson

This report presents 900° C BM-AGA carbonization and related data for coals from the principal beds of Nicholas, Randolph, and Webster Counties, W. Va. Thirty-three samples from nine coal beds in three counties were car-bonized at 900° C in the l8-inch-diameter BM-AGA retort, data from which have been correlated with industrial production. Host of the samples were chemically suitable for metallurgical use, and their coking properties were satisfactory. Except for four of the Lower Kit-tanning samples, the ranges of constituents in the coal seams were 1.8 to 9.0 percent ash and 0.4 to 1.1 percent sulfur, values within the range of accept-ability for metallurgical coals. Coke strength indexes were normal for Appalachian coals of similar rank, and the tumbler stability indexes of the coke ranged from 35 to 57.

Jan 1, 1969

By A. A. Cochran

Bureau of MinesThe Bureau of Mines studied the development of practical methods for recovering manganese from the extensive domestic resources of low-grade ores and open hearth slags. A one-step operation was developed on a laboratory scale in which manganese and iron compounds are treated with chlorine, volatilized, and separated by selective condensation. Manganese recoveries of 90 to nearly 100 percent were obtained from 9 of the most important domestic ores. Analyses of the manganese chloride product indicated that it was suit-able for aqueous electrolysis with little additional purification. A complete, integrated process that provides for the recovery and recycling of chlorine is proposed. This process appears to have distinct advantages over previously proposed manganese recovery processes, and, in sharp contrast to leaching procedures, it is applicable to practically any manganese-bearing material.

Jan 1, 1967

By A. Gene Collins

This report discusses some of the chemistry and geochemistry of cesium and rubidium. Knowledge of the cesium and rubidium content of oilfield waters aids in resolving the origin of waters and petroleum, exploring for petroleum and other valuable minerals, discovering water pollution sources, and augmenting the knowledge of geologic formations. The methods described in this report permit the detection of less than 0.01 mg/l of cesium and/or rubidium in a complex oilfield brine or water. Solvents possessing high-dielectric constants were evaluated for their ability to extract cesium and rubidium tetraphenylboron from oilfield waters and for their flame emission characteristics. Nitroethane was selected and used for the extraction and flame spectrophotometric determinations because it gave the highest sensitivity. Cesium 137 and rubidium 86 were used to determine the extraction efficiencies, which were about 87 percent and 58 percent respectively using a single 10 ml nitroethane extraction from a distilled water matrix. The standard deviation of the determination was 0.0008 mg for cesium and 0.0007 mg for rubidium in the 0.01 mg range.

Jan 1, 1965

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion - exchange X- ray spectrographic method was developed and evaluated for determining trace amounts of cobalt and nickel in high - purity tungsten and tungsten trioxide . The sensitivity for both cobalt and nickel is in the range from 0.2 to 0.5 μg ( 0.04 to 0.1 ppm , based on 5 gram samples ) . Accuracy at the 5 to 20 μg level is ±10 percent of the amount present . Approximately 16 hours elapsed time is required for analysis

Jan 1, 1963

By F. D. DeVaney

The supply of manganese is a subject of much interest. The idea of obtaining it from rhodochrosite-MnC03 is attractive because the carbonate is supposed not to be so contaminated with impurities as the commonly utilized oxides. Large bodies of rhodochrosite-bearing rock have been known for a long while to exist at Butte, Mont. Hence samples were obtained from that place. In the two samples examined quartz was the chief diluting substance. The leaner sample was about one half quartz; some copper, lead, zinc, and iron sulphides were also present. The rhodochrosite amounted to about 40 per cent, so that the sample had a tenor of about 20 per cent manganese. This sample was the subject of the examination reported herein.

Jan 1, 1928

By William J. Campbell

The purpose of this investigation was to develop a rapid, accurate method of analysis for small amounts of calcium in wolframite concentrates. This analysis is necessary to determine if the wolframite concentrates meet United States National Stockpile Specification P-57R2, which limits the calcium content to 0.2 percent. Because of the small depth of the sample analyzed in fluorescent X-ray spectrography, the calcium Kaline intensity was a function of the chemical composition of the calcium-bearing particle as well as the total matrix composition. This particle-composition effect was particularly important in this analysis, as the calcium may be present as a carbonate, tungstate, phosphate, etc. Three methods of preparing the sample eliminated the variation of calcium Ka intensity with mineralogical occurrence: (1) Reduction in particle size by extensive grinding, (2) chemical fusion with sodium carbonate, and (3) solution of the calcium by an acid attack.

Jan 1, 1958

By Larry A. Haas

A major problem encountered in dump leaching operations is the plugging of both the dump and the piping by precipitated iron compounds. Bureau of Mines research to obtain basic data on agitation leaching and dump leaching methods has shown that the addition of organic chelating reagents can significantly enhance the lixiviant permeability through the ore and the concentration of the metal values in the liquor. For example, the addition of 5 giL citric acid (CA) to a conventional sulfuric acid lixiviant almost doubled the fluid flow rate through 5-cm-diameter laboratory columns containing copper ore. After 185 h of per-colation leaching, the metal concentrations with (and without, in parentheses) CA were 1.7 (1.5) giL Cu, 200 (70) ppm Mn, 160 (40) ppm AI, and 6 (3) ppm Co. The enhancement of metal concentrations with chelating reagents such as CA was confirmed by determining the solubil-ity of several metal ions as functions of pH and chelating reagent con-centration. When ferric ions became insoluble at pH values above 3, the concentrations of other ions also decreased. The addition of che-lating reagents kept iron, as well as the other dissolved metals, in solution even at pH values as high as 5. Citric acid was a more effective chelating reagent than gluconic acid, oxalic acid, or sodium lignin sulfonate.

Jan 1, 1985

By Ronald H. Church

As part of the Bureau of Mines health and safety research program in strata control, a ground-penetrating radar (GPR) system capable of pene-trating approximately 10 ft into the mine roof has been devised to identify anomalistic conditions. The GPR system consists of a transmitter with carrier frequencies of 250, 500, and 1,000 MHz, utilizing a dipole antenna, and a receiver, consisting of a dipole antenna fed into a sampler with a time base housed in a storage oscilloscope. A computer was utilized for data acquisition and data processing. Data analysis by computer enhancement revealed recognizable return ra-dar signatures from the middle man rock and main roof of the test site. These stratigraphic anomalies can be cataloged for recognizable fea-tures, which from the past history of the mine may have been shown to create strata control problems. Early recognition of such features could lead to immediate corrective actions and result in the saving of lives.

Jan 1, 1985

By Milton H. Fies

The dedication of thin building, establishing a station of the U.S. Bureau of vines at the University of Alabama, bristles with significance and challenges the wisdom and courage of the people of this State. Here is united, in common aim, the Engineering School of our State University, recognized for its competency and usefulness, and the Federal Bureau of Mines. The Bureau is one of the most effective arms of our National Government. It outranks in accomplishment, measured by practical scientific contribution, any like governmental organization in all the other nations. It possesses none of the characteristics of many other bureaus of government which have created popular bias. Here is one Bureau devoid of political suggestion or aim with a personnel zealously devoted to labor in scientific re¬search - an organization marked by practical accomplishment, alleviating many of life's burdens, raking easier life's pathway, and unerringly pointing to life's possibilities.

Jan 1, 1936

By James M. Nishi, Lloyd Carpenter

Sixteen elements were determined spectrochemically in the general range of 3 to 1,000 ppm in high - purity columbium . Samples were converted thermally to Cb2 O , mixed with graphite and Ge02 , and excited for 15 seconds using a 15 - ampere dc arc . For the molybdenum determination , the oxidized samples were mixed with NaCl and Geo₂ and excited for 30 seconds . Spectra were recorded on photographic plates , and spectral line transmittance values were measured photometrically . Relative - intensity ratios of selected analytical and internal standard spectral lines were plotted against concentrations of standards to form curves from which concentrations of impurities were read . Average precision of the method was 11.2 percent relative standard deviation .

Jan 1, 1964

By Fieldner. A. C.

"In preparing this paper, an attempt was made to obtain results of plant-scale carbonization tests on washed and unwashed coal tram to same mine. A letter. in which the following questions were asked, was sent to some 50 coke-oven superintendents and others who might be interested:“What is the influence of washing coal on:(1) The chemical and physical properties of coke, as for example, the size, the amount of breeze, the fracture, strength, cell-structure, etc.(2) The quantity and quality of gas and by-products.(3) The capacity of the ovens.(4) The composition of the coal..""Your general opinion, as well as any specific data or results of testa, on this important subject will be greatly appreciated.""Of the 45 replies received, 24 stated that they had never used washed coal; 11 had used washed coal but had no comparative data on similar coals washed and unwashed; 7 answered some of the questions based on their general experience; and 3 gave some test data on Pittsburgh bed coal from western Pennsylvania. In none of the three tests did the washed coal come from the same mine as the unwashed. The washed coals in the three tests were from the same washery - one of modern construction in which the operations are under careful technical control in order to give a uniform product containing a minimum of surface moisture. The unwashed coals which were previously used in these plants were from different nearby mines in the same coal bed, and were supplied by the same company. Obviously, no sweeping or finale conclusions can be drawn from these few tests on coal from a single washery. Therefore, the writer vas obliged to consult the literature, coal-carbonization and coal-washing engineers, and other authorities to supplement the fragmentary information gleaned from the questionnaires in order to present a picture of chat gas engineers may expect from the use of washed coal in a carbonizing plant."

May 1, 1930

By L. R. Burdick

This paper presents a review of published investigation dealing with the importance of sulfur compounds in the deterioration of materials or providing some basis for estimating the extent of loss shareable to such air pollution. Materials included are cement, stone, metals, paint, leather, paper, sand cloth. The investigations may be divided into two classes, one of the laboratory type in which the sulfur content and the humidity of the air were controlled and the other dealing with the exposure of materials to atmospheres not under control. The first type of work has shown that cement is subject to deterioration by the action of sulfur dioxide gas. The experiments with stone indicate that although limestone takes up sulfur dioxide, from the air, moist sulfur dioxide-air mixtures alone cannot be used for establishing- the comparative weathering- qualities of the different types of stone by accelerated test methods. Laboratory tests indicate that sulfur compounds in the air accelerate the corrosion of iron, steel, zinc, copper, and nickel at normal air temperatures and at certain relative humidities. It has also been indicated that certain types of paint are, affected by high sulfur dioxide concentrations, and that paper is attacked by sulfur dioxide in the atmosphere. The investigations of the second type show the amount or variation of corrosion in different localities and under different types of exposure. The investigations (10) (18)4/ during which sulfur determinations were made indicate that sulfur dioxide is a main controlling factor in the corrosion of iron and steel but according to Quick (18) may not be for some nonferrous metals. In general, the laboratory tests do not Jive definite data on the loss due to sulfur compounds at the concentrations normally found in the air. The data from atmospheric exposures are not complete from the standpoint of the exact effect of the sulfur compounds. Damage to materials so exposed is affected by factors such as other chemical contaminants, humidity, rainfall, solid deposits, and sunlight. A simple scheme has been devised in Great Britain which is considered to provide a measure of the attack of sulfur compound, on building materials (1). Small cylinders coated

Jan 1, 1939

By S. H. Ash

The paramount responsibility of Government is to protect the general welfare. One of the chief functions of the Bureau of Mines is to investigate and publicize methods of increasing safety and efficiency in mining operations. In an industrial civilization, energy resources constitute the foundation of a sound economic structure (14).4/ Coal is only one source of energy, but it provides more than half the energy consumed in the United States.

Jan 1, 1946

By D. J. MacDonald

As part of a U.S. Bureau of Mines program seeking improvements to the Bayer process, a typical Jamaican bauxite was heated at temperatures up to 500° C in hydrogen, and its leachability under Bayer process conditions was measured and properties of its leached residue were observed. The objectives were to find ways to decrease the amount of organic carbon in bauxite or in leach liquor derived from it without impairing its leachability, and to improve the leached residue's filterability. Techniques employed included heating bauxite under pressure in an autoclave with hydrogen, and in flowing hydrogen at ambient pressure in a tube furnace. Leaching tests were done with a 600-mL stirred reactor. In some of the leaching tests, ferrous sulfate (FeS04) was introduced before leaching to produce a partially magnetic product. Results showed that exposure to hydrogen at temperatures from 160° to 360° C progressively diminished the bauxite's content of organic carbon and decreased the ratio of organic carbon to aluminum in leach liquor, an improvement that would allow a process using hydrogen-treated bauxite to be operated at a smaller recycle ratio, thereby consuming less energy and allowing greater throughput for a plant of given capacity. The bauxite's leachability was not impaired by high-temperature pretreatments, except at temperatures higher than 280° C. Pretreatments in hydrogen produced black, partially reduced bauxite which upon leaching gave a residue that was attracted to a magnetic field and was amenable to separation from green liquor by a magnetic filtration method.

Jan 1, 2010

By G. R. Peterson

The Bureau of Mines evaluated the potential supply of cobalt from known domestic resources, both as a primary product from some deposits and as a byproduct from others, and found that U.S. production could play an important role in meeting U.S. cobalt needs by the mid-1980's. This production would be of a relatively short duration, however, with production declining significantly before the year 2000. As part of the study, a tonnage-price relationship was developed indicating the quantity of cobalt that could be produced from known cobalt-bearing deposits at various primary commodity prices and at a 15-percent rate of return on the required capital investment. All capital and operating costs are calculated in August 1980 dollars, and commodity prices are based on August 1980 prices. Known U.S. cobalt-bearing deposits which represent the current U.S. cobalt reserve base contain some 310,800 metric tons of cobalt in slightly over 1 billion metric tons of demonstrated mineralized material. Approximately 37 percent of the cobalt contained in the reserve base is considered recoverable using existing technology. Of this quantity, some 87,000 metric tons of cobalt is economically recoverable assuming a cobalt price of $25 per pound, a copper price of $1 per pound, and a lead price of $0.40 per pound. Assuming that the cobalt price decreases to $15 per pound, keeping copper and lead prices constant, the quantity that is considered economically recoverable declines to some 45,700 metric tons. Domestic cobalt consumption in 1979 was 7,900 metric tons (17.4 million pounds). Currently, no primary cobalt is produced from domestic resources, and none has been produced since 1971.

Jan 1, 1981

By Charles B. Kenahan

Vanadium is subject to only light corrosion in phosphoric acid at temperatures up to 60° C. and has a moderate corrosion rate in this acid at 100° C. It is relatively corrosion resistant in sulfuric and hydrochloric acids up to 60° C, but corrodes rapidly at 100° C. It corrodes rapidly in dilute nitric acid at 35° C. Vanadium is almost inert in 10-percent solutions of formic, acetic, lactic, tartaric, and citric acids; in 9-percent oxalic acid it corrodes slowly up to 60° C. and rapidly at 100° C. Vanadium is resistant to corrosion in substitute ocean water, tapwater, and in 3-percent sodium chloride and 10-percent sodium hydroxide solutions. It is readily attacked, however, by 20-percent ferric chloride, 20-percent cupric chloride and 5-percent mercuric chloride solutions. Vanadium is protected by contact with magnesium, aluminum, and steel SAE 4130 in substitute ocean water, by magnesium and aluminum in 3-percent sodium chloride solution, and by magnesium in tapwater. Vanadium protects copper in substitute ocean water. When vanadium and stainless steel are coupled in sulfuric acid solutions, both metals are usually unaffected by contact, whereas the corrosion rate of titanium in sulfuric acid is greatly reduced by contact with vanadium.

Jan 1, 1962